Reaction equation
Br[CH2:2][C:3]1[CH:7]=[C:6]([C:8]2[S:9][C:10]([Cl:13])=[CH:11][CH:12]=2)[O:5][N:4]=1.C1N2CN3CN(C2)C[N:15]1C3.Cl>CCO>[Cl:13][C:10]1[S:9][C:8]([C:6]2[O:5][N:4]=[C:3]([CH2:2][NH2:15])[CH:7]=2)=[CH:12][CH:11]=1Participants
5
Procedure
1.00 g (3.59 mmol) 3-Bromomethyl-5-(5-chloro-thiophen-2-yl)-isoxazole and 503.3 mg (3.59 mmol) urotropin were dissolved in 40 mL EtOH. The reaction mixture was stirred at room temperature for 16 h. The next day 3 mL of a conc. HCl-solution were added and the resulting mixture was refluxed for 45 minutes. After cooling the precipitate was filtered off and washed with water. The white crystalline material was dried under reduced pressure at 40° C.
Workup
- temperaturethe resulting mixture was refluxed for 45 minutes
- temperatureAfter cooling the precipitate
- filtrationwas filtered off
- washwashed with water
- customThe white crystalline material was dried under reduced pressure at 40° C.
Sources & evidence
- ORD record
- ord-5a6c7457cfdb4e10b5a9e271bd261c05
- Source dataset
- uspto-grants-2010_06
- Patent number
- US07741341B2
Linked notes
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